CN104548647A - Multipoint reciprocating continuous crystallizer - Google Patents

Multipoint reciprocating continuous crystallizer Download PDF

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Publication number
CN104548647A
CN104548647A CN201510040508.9A CN201510040508A CN104548647A CN 104548647 A CN104548647 A CN 104548647A CN 201510040508 A CN201510040508 A CN 201510040508A CN 104548647 A CN104548647 A CN 104548647A
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rectifying
crystallizer
crystallized region
heating
crystallization
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CN201510040508.9A
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Chinese (zh)
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CN104548647B (en
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易争明
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湘潭大学
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Abstract

The invention provides a multipoint reciprocating continuous crystallizer. The multipoint reciprocating continuous crystallizer is of a U-shaped twin-tower structure, and comprises a feeding hole, a purification section, a melting section, a crystallization section, a heating element, a drain outlet, a discharge hole and a residual liquid outlet; the purification section is located in the tower body on one side of the crystallizer, while the crystallization section is located in the tower body on the other side; the melting section is located at the bottom of the crystallizer; the feeding hole is located at the upper part of the purification section, while the discharging hole is located on one side of the bottom of the melting section and the drain outlet is located on the other side of the bottom of the melting section; a cooling jacket is arranged outside the crystallization section, and a coolant goes in at the top and out at the bottom; a heating jacket is arranged outside the purification section, and a heating agent goes in at the bottom and out at the top; the heating element is located in the melting section; a stirring shaft and a spiral stirrer are arranged in the crystallization section and the purification section; the temperature distribution, the crystal crystallization rates and the crystal bed layer heights of the purification section and the crystallization section are controlled by controlling the temperatures and the flow rates at a heating agent inlet and a coolant inlet. The multipoint reciprocating continuous crystallizer is capable of enhancing the effect of countercurrent washing in the crystallizer, improving the mass transfer efficiency and greatly improving the purification efficiency.

Description

The reciprocating continuous crystalizer of multiple spot

Technical field

The present invention relates in a kind of industrial crystallization organic separator of purifying, particularly provide a kind of novel melting crystallisation and prepare high-purity crystallized separator.

Background technology

What currently marketed a lot of chemical products faced is production capacity surplus, therefore improving technique, and the purity and the minimizing producing cost that improve product become the task of top priority.The purity that fusion-crystallization improves product as a kind of organic method of separating-purifying of high-efficiency low energy consumption when reducing production cost is subject to each enterprises pay attention day by day.

Fusion-crystallization is the process that realization is separated according to freezing point between separate substance is different.And owing to not using solvent in fusion-crystallization, do not need solvent removal and recovery, and there is no the pollution that solvent brings, and less to the size relative requirement of equipment; The operating temperature of fusion-crystallization depends on the fusing point of crystalline material, therefore without the need to very high operating temperature, require less for heating system, in general, energy consumption is equivalent to 1/3 of rectifying, and is less than traditional rectifying separation process for the mechanical strength of equipment and the requirement of pressure rating.

In fusion-crystallization, it is generally acknowledged three large factors affect crystallization efficiency and product purities: be recrystallized, perspiration, countercurrent washing, wherein countercurrent washing acts in three large factors and plays an important role.Countercurrent washing effect refers in the crystal bed of purifying column, when crystal is in time adhering to sedimentation downwards together with liquid, contact with phegma upwards, owing to there is concentration difference between phegma and attachment liquid, therefore there is Convention diffusion between, thus achieve quality transmission, crystal purity is improved and plays an important role.

Numerous domestic enterprise is all promoting the crystallizer type of oneself being good at, but more rare breakthrough innovation.Crystallizer is mainly for crystallization process provides a good platform to meet the condition required for crystal growth.So exploitation is efficient, stable, energy-conservation novel crystallization device has its necessity.

In traditional crystallizer, because the restriction of mold structure, no matter be by changing operating condition (as changed reflux ratio) or change tower inner structure change (controlling phegma trend), often can not having very large lifting for countercurrent washing effect.Therefore, be necessary that technological improvement is carried out in the direction from improving mold structure.

Summary of the invention

The object of the invention is to overcome the deficiencies in the prior art, provide a kind of novel melting crystallisation and prepare high-purity crystallized device, this device can improve the effect of countercurrent washing in crystallizer, improves mass-transfer efficiency and significantly can improve the purification efficiency of crystal.

The invention provides the reciprocating continuous crystalizer of a kind of multiple spot, this Latent Heat described is U-shaped Double-Tower Structure, comprises charging aperture (11), rectifying section (14), melt zone (15), crystallized region (4), heating element heater (10), sewage draining exit (16), discharging opening (5) and raffinate outlet (1); Wherein rectifying section (14) is positioned at the side tower body of crystallizer, crystallized region (4) is positioned at the opposite side tower body of crystallizer, melt zone (15) is positioned at the bottom of crystallizer, and side is connected with rectifying section (14), opposite side is connected with crystallized region (4); Rectifying section (14) and crystallized region (4) inside are equipped with the melt zone (15) that agitating device passes to crystalliser feet; Rectifying section (14) outside is provided with heater, and crystallized region (4) outside is provided with cooling device; Charging aperture (11) is positioned at rectifying section (14) top, discharging opening (5) is positioned at the side, melt zone (15) bottom be connected with crystallized region (4), and sewage draining exit (16) is positioned at melt zone (15) the bottom opposite side be connected with rectifying section (14); Heating element heater (10) is positioned at melt zone (15).

The heater of foregoing purification section (14) outer setting be heater strip, heating tape or heating jacket (13) any one.

Wherein the middle heating agent entrance (9) of the heating jacket (13) of the heater of foregoing purification section (14) outer setting is positioned at the bottom of rectifying section (14), heating agent outlet (12) is positioned at the top of rectifying section (14), by controlling the temperature of heating agent entrance (9) and flow to control the Temperature Distribution of rectifying section (14), crystal structure speed and crystal bed height.

The cooling device of aforementioned crystalline section (4) outer setting is cooling jacket (3), the coolant entrance (2) of cooling jacket (3) is positioned at the top of crystallized region (4), coolant outlet (8) is positioned at the bottom of crystallized region (4), by the temperature of controlled cooling model entrance (9) and flow with the Temperature Distribution of crystallization control section (4), crystal structure speed and crystal bed height.

Described agitating device is shaft (6) and agitator disposed thereon.

Wherein the upper agitator arranged of shaft (6) is preferably spiral agitator (7).

Advantageous Effects of the present invention is embodied in, the motive force that in crystallizer countercurrent washing in the past, phegma is not additional, and is single reflow washing.And the present invention uses novel U-shaped structural design in crystallizer, change back and forth crystallized region, rectifying section crystal bed potential difference to change in crystallizer fused solution backflow direction, repeatedly back and forth carry out countercurrent washing effect at crystallized region, rectifying section, increase the countercurrent washing effect of solid-liquid two-phase, accelerate the renewal of the heat and mass transport boundary of crystal and mother liquor, therefore, its mass-transfer efficiency, refining effect are higher than fractional crystallization tower existing on market.

In U-shaped crystallizer, crystal is separated out and can be formed crystal bed at double tower, and the thickness of bed determines the pressure drop of two towers, controls the pressure reduction between two towers, under certain pressure reduction, forces to promote phegma and crystal countercurrent washing.Repeatedly adjust pressure differential, liquid phase in tower is moved back and forth between double tower, repeatedly mass transfer effect can be reached.

The factor affecting crystallization mainly contains perspiration, recrystallization, countercurrent washing effect, this crystallizer is U-shaped design, mainly countercurrent washing effect is strengthened, the washing of single is transferred to washing repeatedly, and a kind of potent motive force (pressure reduction) in addition.Because reflux back and forth, crystal repeatedly transfers fused solution to, and counterweight crystallization effect has certain enhancing.

The formation of crystal is relevant with temperature and stir speed (S.S.), and in adjustment chuck, the temperature of cooling agent or heating agent and flow can control the temperature in double tower, thus the amount of crystals controlled in the tower of both sides and thickness.Because crystal free settling is comparatively slow relative to the forced refluence of this crystallizer, therefore uses spiral agitator to carry, crystal also can be prevented too intensive and solidify.

Accompanying drawing explanation

Fig. 1 is the structural representation of the reciprocating continuous crystalizer of multiple spot.

Implication represented by Reference numeral is: raffinate outlet 1, coolant entrance 2, cooling jacket 3, crystallized region 4, discharging opening 5, shaft 6, spiral agitator 7, coolant outlet 8, heating agent entrance 9, heating element heater 10, charging aperture 11, heating agent outlet 12, heating jacket 13, rectifying section 14, melt zone 15, sewage draining exit 16.

Detailed description of the invention

Adopt the reciprocating continuous crystalizer of multiple spot of the present invention (as shown in Figure 1), material enters crystallizer rectifying section 14 from charging aperture 11, flows to raffinate outlet 1.Be provided with heating jacket 3 outside rectifying section 14, chuck heating agent feed postition is bottom in and top out, and rectifying section 14 temperature is raised from top to bottom gradually.After material adds, to mix in former tower crystallize out after liquid phase, control to enter the temperature of chuck heating agent entrance 9 and flow to control rectifying section 14 Temperature Distribution, form certain crystal bed at rectifying section 14, use shaft 6 and spiral agitator 7 to be carried to melt zone 15 by crystal.In this process, rectifying section 14 Temperature Distribution of controlling well is significant for crystallization perspiration.After material enters melt zone 15, crystal all melts rear formation fused solution and flows into crystallized region 4, and be provided with cooling jacket 3 outside crystallized region 4, cooling agent feed postition is upper entering and lower leaving, and crystallized region 4 temperature is reduced from top to bottom gradually.In the process of flow direction of material raffinate outlet 1, high-solidification point component is constantly separated out with crystal state and is recovered and sedimentation from liquid phase, this process can form certain crystal bed at crystallized region, the content of liquid phase high-solidification point component wherein when arriving outlet is minimized the level to expection, then gets rid of from raffinate outlet 1 as raffinate (or claiming lean solution).Crystal sedimentation enters melt zone 15 and forms fused solution, after crystallized region 4, rectifying section 14 have certain crystal bed height respectively, by controlling to enter the heating agent of chuck or coolant temperature and flow to control Crystallization speed and crystal bed height causes pressure differential between double tower, directly directly can carry out supercharging, decompression operation in rectifying section, crystallized region tower top, when crystallized region 4 pressure is higher than rectifying section 14 pressure, fused solution is refluxed and enters rectifying section 14, carry out counter flow action with the crystal of rectifying section 14 sedimentation downwards.Change the pressure differential between two towers afterwards, make fused solution reenter crystallized region 4, carry out countercurrent washing effect with sedimentation crystal.Repeatedly repeatedly change pressure reduction, carry out countercurrent washing repeatedly, obtain a highly purified fused solution part and discharge from discharging opening, another part carries out countercurrent washing effect as phegma.

Claims (7)

1. the reciprocating continuous crystalizer of multiple spot, it is characterized in that, described Latent Heat is U-shaped Double-Tower Structure, comprises charging aperture (11), rectifying section (14), melt zone (15), crystallized region (4), heating element heater (10), sewage draining exit (16), discharging opening (5) and raffinate outlet (1); Wherein rectifying section (14) is positioned at the side tower body of crystallizer, crystallized region (4) is positioned at the opposite side tower body of crystallizer, melt zone (15) is positioned at the bottom of crystallizer, and side is connected with rectifying section (14), opposite side is connected with crystallized region (4); Rectifying section (14) and crystallized region (4) inside are equipped with the shaft (6) passing to crystalliser feet melt zone (15) and the ribbon blender being arranged at this shaft (6) upper band inclination angle; Rectifying section (14) outside is provided with heater, and crystallized region (4) outside is provided with cooling device; Charging aperture (11) is positioned at rectifying section (14) top, discharging opening (5) is positioned at the side, melt zone (15) bottom be connected with crystallized region (4), and sewage draining exit (16) is positioned at melt zone (15) the bottom opposite side be connected with rectifying section (14); Heating element heater (10) is positioned at melt zone (15).
2. crystallizer according to claim 1, is characterized in that, the heater of described rectifying section (14) outer setting is any one in electrical heating wire, heating tape or heating jacket (13).
3. crystallizer according to claim 2, it is characterized in that, the heating agent entrance (9) of the heating jacket (13) of described rectifying section (14) outer setting is positioned at the bottom of rectifying section (14), heating agent outlet (12) is positioned at the top of rectifying section (14), by controlling the temperature of heating agent entrance (9) and flow to control the Temperature Distribution of rectifying section (14), crystal structure speed and crystal bed height.
4. the crystallizer according to claim 1-3 any one, is characterized in that, the cooling device of described crystallized region (4) outer setting is cooling worm or cooling jacket (3).
5. crystallizer according to claim 4, it is characterized in that, the coolant entrance (2) of the cooling jacket (3) of described crystallized region (4) outer setting is positioned at the top of crystallized region (4), coolant outlet (8) is positioned at the bottom of crystallized region (4), by the temperature of controlled cooling model entrance (9) and flow with the Temperature Distribution of crystallization control section (4), crystal structure speed and crystal bed height.
6. the crystallizer according to claim 1-5 any one, is characterized in that, described in be arranged on shaft (6) blade formula agitator angle of inclination be 5 ~ 10 °.
7. crystallizer according to claim 6, is characterized in that, described in the agitator be arranged on shaft (6) be spiral agitator (7).
CN201510040508.9A 2015-01-27 2015-01-27 The reciprocating continuous crystalizer of multiple spot CN104548647B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2603667A (en) * 1950-01-26 1952-07-15 Phillips Petroleum Co Fractional crystallization
US2659761A (en) * 1948-08-23 1953-11-17 Dow Chemical Co Fractional crystallization method
CN2834659Y (en) * 2005-11-25 2006-11-08 四川大学 Apparatus for preparing high-purity organism by fusion crystallization method
CN203989946U (en) * 2014-08-29 2014-12-10 上虞市临江化工有限公司 A kind of double hose intersect mixed flow crystallization apparatus

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2659761A (en) * 1948-08-23 1953-11-17 Dow Chemical Co Fractional crystallization method
US2603667A (en) * 1950-01-26 1952-07-15 Phillips Petroleum Co Fractional crystallization
CN2834659Y (en) * 2005-11-25 2006-11-08 四川大学 Apparatus for preparing high-purity organism by fusion crystallization method
CN203989946U (en) * 2014-08-29 2014-12-10 上虞市临江化工有限公司 A kind of double hose intersect mixed flow crystallization apparatus

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